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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 505 records · Page 28
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Constraints in Semicrystalline Polymers: Using Quasi-isothermal Analysis to Investigate the Mechanisms of Formation and Loss of the Rigid Amorphous Fraction

The nanoscale phase behavior of a semicrystalline polymer is important for mechanical, thermal, optical and other macroscopic properties and can be analyzed well by thermal methods. Using quasi-isothermal (QI) heat capacity measurements, we investigate the formation behavior of the crystalline, mobile amorphous, and rigid amorphous fractions in poly(trimethylene terephthalate), PTT. The crystal and rigid amorphous phases comprise the total solid fraction in PTT at temperatures above T{sub g}, the glass transition temperature of the mobile amorphous fraction. PTT was quasi-isothermally cooled step-wise from the melt which causes its crystalline fraction to be fixed below 451 K. Between the high temperature fulfillment of the T{sub g} step and 451 K, the temperature dependent rigid amorphous fraction (RAF) is completely determined. For PTT, most of the RAF vitrifies between 451 K and T{sub g} step by step during QI cooling after the crystals have formed. The constraints imposed by the crystal surfaces reduce the mobility of the highly entangled polymer chains. We suggest the vitrification of RAF proceeds outward away from the lamellar surfaces in a step by step manner during QI cooling. Upon reheating, devitrification of RAF occurs at a temperature above its previous vitrification temperature, due to the effects of densification brought by physical aging during the long period of quasi-isothermal treatment. Finally, we consider recent concepts related to jamming, which have been suggested to apply to filled polymer systems, and may also be applicable in describing constraints exerted by crystal lamellae upon the RAF.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Crosslinked Matrimid®-like polyimide membranes with unimodal network structure for enhanced stability and gas separation performance

Gas separation membranes have attracted academic and industrial attention, and crosslinking has been identified to be one of the most effective ways to enhance membrane stability. In this paper, a series of crosslinked Matrimid®-like films with unimodal network structures are prepared via thermally end-linking phenylethnyl-terminated BTDA-DAPI oligomers with well-controlled molecular weight (i.e., 3000–15,000 g/mol), wherein the crosslink density (the inter-crosslink chain length) of resulting unimodal networks is systematically varied by using oligomers with various molecular weight. Comprehensive characterizations of chemical structure, thermal properties, microstructures are performed. Pure-gas permeation measurements are performed focusing on H 2 /CH 4 and CO 2 /CH 4 separations as a function of crosslink density. In sharp contrast to the commonly observed permeability reduction in randomly crosslinked networks, all the crosslinked unimodal films, even when densely crosslinked, present markedly enhanced permeability and well-maintained ideal selectivity relative to the uncrosslinked linear counterpart, leading to almost horizontal movements towards upper bounds along with expectedly enhanced membrane stability. In conclusion, it is concluded that introducing bulky groups at the crosslink sites provide a practical means to counteract the densification effect induced by crosslinking and the construction of unimodal networks exemplifies a fundamentally new strategy to regulate the microstructure and property of crosslinked membranes for gas separations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Compression behavior of microcrystalline cellulose spheres: Single particle compression and confined bulk compression across regimes

Particle characteristics can drastically influence the process-structure-property-performance aspects of granular materials in compression. In this study, we aim to computationally simulate the mechanical processes of stress redistribution in compacts including the kinematics of particle rearrangement during densification and particle deformation leading to fragmentation. Confined compression experiments are conducted with three sets of commercial microcrystalline cellulose particles nearly spherical in shape with different mean particle size. Experimentally measured compression curves from tall powder columns are fitted with the Kenkre et al. (J. of American Chemical Society, Vol. 79, No. 12) model. This model provides a basis to derive several common two-parameter literature models and as a framework to incorporate statistical representations of critical particle behaviors. We focus on the low-stress compression data and the model comparisons typically not discussed in the literature. Furthermore, additional single particle compressions report fracture strength with particle size for comparison to the apparent particle strength extracted from bulk compression data.

42 ENGINEERING↗
DOE OSTI2021

Effects of different pelleting technologies and parameters on pretreatment and enzymatic saccharification of lignocellulosic biomass

Densification of lignocellulosic biomass is beneficial for its logistics, and in some situations, also for its application in biorefineries. In this study, industrial pellets and laboratory-made pellets produced at different die temperatures (90, 125 °C) from wheat straw, beech, and pine were pretreated (by dilute acid and alkali) and enzymatically hydrolyzed to study the effects of pelleting on pretreatment and sugar yield. The results showed that industrial pelleting positively affected sugar yield of the three biomasses for both acid and alkaline pretreatments, while laboratory pelleting affected sugar yield differently related to pretreatment types and biomass species. Pelleting disturbed biomass cell wall structure and affected the stability of hemicellulose and β-O-4' linkages in lignin. The extent of hemicellulose solubility during acid pretreatment and the amount of lignin β-O-4' ether linkages present in acid pretreated substrates could serve as indicators of the effect of pelleting on sugar yield. The structural modifications caused by pelleting and their effects on the enzymatic sugar yield correlate tightly to pelleting technology, pretreatment method, and biomass species. As a result, the discrepant effects between industrial and laboratory pelleting on sugar yield observed in this study should be considered when designing future studies.

09 BIOMASS FUELS↗
DOE OSTI2018

Anisotropic lattice expansion determined during flash sintering of BiFeO 3 by in-situ energy-dispersive X-ray diffraction

BiFeO 3 has a Curie temperature (T C ) of 825 °C, making it difficult to sinter with conventional methods while maintaining the purity of the material, as unavoidably secondary phases appear at temperatures above T c . Flash sintering is a relatively new technique that saves time and energy compared to other sintering methods. BiFeO 3 was flash sintered at 500 °C to achieve 90% densification. In-situ energy dispersive X-ray diffraction (EDXRD) reflected that the material did not undergo any phase transformation, having been sintered well below the T C . Interestingly, anisotropic lattice expansion in the materialwas observed when the sample was exposed to the electric field.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Reactive flash sintering of the complex oxide Li 0.5 La 0.5 TiO 3 starting from an amorphous precursor powder

We report the transformation of an amorphous mixture of Li 0.5 La 0.5 TiO 3 (LLTO) directly into a single phase dense polycrystal, all within a few seconds at about 800°C by the flash method. The starting material is a chemically-prepared precursor powder that experiences concurrent crystallization and densification to cubic LLTO during the flash event, as shown by in-situ X-ray measurements. The experiments were conducted at a constant heating rate with fields from 80 to 120 V cm –1 and a current limit of 60 mA mm –2 . Here, the resulting polycrystal yielded a bulk conductivity of 0.5 mS cm –1 .

36 MATERIALS SCIENCE↗
DOE OSTI2025

Induction ultrafast sintering

This study proposes and demonstrates induction ultrafast sintering (IUS), which enables rapid densification of refractory and other materials via two contactless modalities: direct IUS (d-IUS), where heating occurs through electromagnetic coupling with the sample, and susceptor IUS (s-IUS), where heating is achieved indirectly via an induction-heated metal case. Ultrahigh heating rates of ∼75 to >450 °C/s and temperatures exceeding 2500 °C are readily achieved. Both d-IUS and s-IUS densify molybdenum to high densities within 120 s, with only ∼1–3 % porosity observed by image analysis. Similarly, 3 mol % yttria-stabilized zirconia (3YSZ) reaches ∼97 % relative density in 30 s via s-IUS. This study further demonstrates ultrafast reactive sintering of two difficult-to-sinter materials: a refractory compositionally complex alloy–carbide (RCCA–CCC) composite, NbMoTaW–(Nb 0.37 Mo 0.11 Ta 0.39 W 0.13 ) 2 C, using d-IUS, and a compositionally complex silicide (CCS), (Mo 1/3 Nb 1/3 Zr 1/3 )Si 2 , using s-IUS. This IUS platform offers a versatile route for high-throughput materials discovery and energy-efficient fabrication of bulk refractory materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Microstructural and nanomechanical studies of PVD Cr coatings on SiC for LWR fuel cladding applications

The microstructure and nanomechanical properties of pure Cr coatings deposited on SiC with various physical vapor deposition (PVD) methods have been investigated for the mitigation of hydrothermal corrosion of SiC-SiC f (SiC fiber-reinforced SiC matrix) composite fuel cladding in light water reactors (LWR). Cr coatings (4–7 μm thick) were deposited on unbiased SiC substrates using six variants of magnetron sputtering processes: (i) standard (S-DCMS), (ii) pulsed (P-DCMS), (iii) ion-assisted (I-DCMS), and (iv) pulsed ion-assisted direct current magnetron sputtering (PI-DCMS), (v) high-power impulse magnetron sputtering (HiPIMS), and (vi) bipolar HiPIMS (B-HiPIMS). Microstructural characterization and nanoindentation testing were used to evaluate effects of deposition technique on coating microstructure and nanomechanical properties. The application of positive reverse pulses to the sputter target induced coarsening of the columnar grain structure, while ion bombardment of substrates during deposition promoted densification of the coating microstructure. Both effects are exemplified in B-HiPIMS deposition, resulting in a high-density microstructure with compressive residual stress. Material pile-up around nano-indents and plastic work during nanoindentation were analyzed to understand deformation behavior of the coatings. Finally, the results suggest the B-HiPIMS process to be among the promising methods for the deposition of Cr coatings on SiC-SiC f for LWR cladding application.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Persistent Conductivity in Post-Growth Doped ZnO Films Following Pulsed UV Laser Irradiation

Solution and rf sputter deposited doped ZnO films were subjected to cumulative 4-nsec pulses of 355 nm light from a pulsed Nd:YAG laser at fluences between 5 and 150 mJ/cm2. Film densification, change in refractive index, and an increase in conductivity were observed following room temperature irradiation in air, a carbon monoxide reducing environment, or under vacuum. At fluences between 20 and 80 mJ/cm2, the films did not damage catastrophically under irradiation and high visible transparency persisted. The increase in conductivity is attributed to creation of oxygen vacancies and subsequent promotion of free carriers into the conduction band. Effects were most pronounced in films treated in vacuum. All treated films became insulating again upon equilibration in air at room temperature after several days. Films were characterized by means of UV-VIS-NIR transmission spectroscopy, Raman spectroscopy and Hall measurements. Analysis of interference fringes in measured transmission spectra allowed evaluation of optical properties. Raman measurements showed an increase of LO mode intensity with respect to TO mode intensity as the films became more conducting in accord with previous work. Results of this study are not only important for continued development of transparent conducting oxides, but also provide compelling evidence for the role of free carriers as initiators of the laser damage process in these wide bandgap metal oxide films.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Influence of moisture content, particle size and forming temperature on productivity and quality of rice straw pellets

Highlights: • Optimized conditions were determined for the production of rice straw pellets. • The moisture content and forming temperature are key factors. • High quality rice pellets in the lower heating value and durability were produced. - Abstract: A large amount of rice straw is generated and left as much in paddy fields, which causes greenhouse gas emissions as methane. Rice straw can be used as bioenergy. Rice straw pellets are a promising technology because pelletization of rice straw is a form of mass and energy densification, which leads to a product that is easy to handle, transport, store and utilize because of the increase in the bulk density. The operational conditions required to produce high quality rice straw pellets have not been determined. This study determined the optimal moisture content range required to produce rice straw pellets with high yield ratio and high heating value, and also determined the influence of particle size and the forming temperature on the yield ratio and durability of rice straw pellets. The optimal moisture content range was between 13% and 20% under a forming temperature of 60 or 80 °C. The optimal particle size was between 10 and 20 mm, considering the time and energy required for shredding, although the particle size did not significantly affect the yield ratio and durability of the pellets. The optimized conditions provided high quality rice straw pellets with nearly 90% yield ratio, ⩾12 MJ/kg for the lower heating value, and >95% durability.

09 BIOMASS FUELS↗
DOE OSTI2015

Development of a sintering process for recycling oil shale fly ash and municipal solid waste incineration bottom ash into glass ceramic composite

Highlights: • Glass ceramic composite is prepared from oil shale fly ash and MSWI bottom ash. • A novel method for the production of glass ceramic composite is presented. • It provides simple route and lower energy consumption in terms of recycling waste. • The vitrified slag can promote the sintering densification process of glass ceramic. • The performances of products decrease with the increase of oil shale fly ash content. - Abstract: Oil shale fly ash and municipal solid waste incineration bottom ash are industrial and municipal by-products that require further treatment before disposal to avoid polluting the environment. In the study, they were mixed and vitrified into the slag by the melt-quench process. The obtained vitrified slag was then mixed with various percentages of oil shale fly ash and converted into glass ceramic composites by the subsequent sintering process. Differential thermal analysis was used to study the thermal characteristics and determine the sintering temperatures. X-ray diffraction analysis was used to analyze the crystalline phase compositions. Sintering shrinkage, weight loss on ignition, density and compressive strength were tested to determine the optimum preparation condition and study the co-sintering mechanism of vitrified amorphous slag and oil shale fly ash. The results showed the product performances increased with the increase of sintering temperatures and the proportion of vitrified slag to oil shale fly ash. Glass ceramic composite (vitrified slag content of 80%, oil shale fly ash content of 20%, sintering temperature of 1000 °C and sintering time of 2 h) showed the properties of density of 1.92 ± 0.05 g/cm{sup 3}, weight loss on ignition of 6.14 ± 0.18%, sintering shrinkage of 22.06 ± 0.6% and compressive strength of 67 ± 14 MPa. The results indicated that it was a comparable waste-based material compared to previous researches. In particular, the energy consumption in the production process was reduced compared to conventional vitrification and sintering method. Chemical resistance and heavy metals leaching results of glass ceramic composites further confirmed the possibility of its engineering applications.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

High Initial Sputter Rate Found for Vaccinia Virions Using Isotopic Labeling, NanoSIMS, and AFM

High-lateral-resolution secondary ion mass spectrometry (SIMS) has the potential to provide functional and depth resolved information from small biological structures, such as viral particles (virions) and phage, but sputter rate and sensitivity are not characterized at shallow depths relevant to these structures. Here we combine stable isotope labeling of the DNA of vaccinia virions with correlated SIMS imaging depth profiling and atomic force microscopy (AFM) to develop a nonlinear, nonequilibrium sputter rate model for the virions and validate the model on the basis of reconstructing the location of the DNA within individual virions. Our experiments with a Cs+ beam show an unexpectedly high initial sputter rate (~100 um 2 ·nm·pA –1 ·s –1 ) with a rapid decline to an asymptotic rate of 0.7 um 2 ·nm·pA –1 ·s –1 at an approximate depth of 70 nm. Correlated experiments were also conducted with glutaraldehyde-fixed virions, as well as O – and Ga + beams, yielding similar results. Based on our Cs + sputter rate model, the labeled DNA in the virion was between 50 and 90 nm depth in the virion core, consistent with expectations, supporting our conclusions. Virion densification was found to be a secondary effect. In conclusion, accurate isotopic ratios were obtained from the initiation of sputtering, suggesting that isotopic tracers could be successfully used for smaller virions and phage.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Structure and Shape of Surface-Mediated Assembly of Surfactants

Achieving controls on the self-assembly of cationic and block copolymer micelles has significant implications for advancing novel material systems for energy, environmental, and biological applications and for tuning fluid flow behavior in subsurface geologic environments. While it is known that the aggregation of micelles is influenced by the composition of the surrounding fluid, the influence of a solid interface has been less explored. In this study, we probe the organization of cetyltrimethylammonium bromide (CTAB) micelles in the absence and presence of the Pluronic P123 block copolymer and quartz substrate using transmission and grazing-incidence small-angle X-ray scattering measurements and classical molecular dynamics (MD) simulations. In the absence of the quartz interface, CTAB with and without P123 molecules assemble as ellipsoid core–shell micelles. Densification of the core on adding P123 is noted from the decrease in the core radius from 15.9 to 14.6 Å. Here, the presence of a quartz substrate causes the micelles to elongate, which is noted by the emergence of a power-law slope in the low q region (<0.02 Å –1 ). Moreover, in the presence of both P123 and the quartz substrate, the micelle shape changes from ellipsoid core–shell to cylindrical core–shell, and a significantly higher number of aggregates are formed. The higher number of aggregates, and faster aggregation kinetics are linked to the organization of the solvent structures as noted from the MD simulations. These findings demonstrate the effects of adding a block copolymer and including a quartz substrate on the self-assembly of cationic (CTAB) micelles, which can be used to inform the design of functional material systems that harness surfactant chemistries.

42 ENGINEERING↗
DOE OSTI2019

Investigation of Accessible Pore Structure Evolution under Pressurization and Adsorption for Coal and Shale Using Small-Angle Neutron Scattering

Pore structure is an important parameter to quantify the reservoir rock adsorption capability and diffusivity, both of which are fundamental reservoir properties to evaluate the gas production and carbon sequestration potential for coalbed methane (CBM) and shale gas reservoirs. In this study, we applied small-angle neutron scattering (SANS) to characterize the total and accessible pore structures for two coal and two shale samples. We carried out in situ SANS measurements to probe the accessible pore structure differences under argon, deuterated methane (CD 4 ), and CO 2 penetrations. The results show that the total porosity ranges between 0.25 and 5.8% for the four samples. Less than 50% of the total pores are accessible to CD 4 for the two coals, while more than 75% of the pores were found to be accessible for the two shales. This result suggests that organic matter pores tend to be disconnected compared to mineral matter pores. Argon pressurization can induce pore contraction because of the mechanical compression of the solid skeleton in both the coal and shale samples. Hydrostatic compression has a higher effect on the nanopores of coal and shale with a higher accessible porosity. Both methane and CO 2 injection can reduce the accessible nanopore volume due to a combination of mechanical compression, sorption-induced matrix swelling, and adsorbed molecule occupation. CO 2 has higher effects on sorption-induced matrix swelling and pore filling compared to methane for both the coal and shale samples. Gas densification and pore filling could occur at higher pressures and smaller pore sizes. In conclusion, the compression and adsorption could create nanopores in the San Juan coal and Marcellus shale drilled core but could have an opposite effect in the other samples, namely, the processes could damage the nanopores in the Hazleton coal and Marcellus shale outcrop.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2025

Nondestructive In Operando Imaging of Thin Film Composite Membrane Compaction Enhanced by AI-Based Segmentation

Reverse osmosis (RO) membranes are essential for desalination and water reuse, yet their permeability declines in high-pressure applications due to membrane compaction. This study investigates the structural and functional responses of commercial brackish, seawater, and high-pressure RO membranes at applied pressures up to 120 bar using a multiscale, nondestructive in operando scanning electron microscopy (iSEM) imaging platform. The iSEM technique reveals progressive densification across the composite membrane structure, which correlates with observed declines in water and solute permeance. To quantify these structural changes with greater fidelity, we combined X-ray computed tomography with AI-based segmentation enabling precise analysis of pore size distribution and thickness of the polysulfone support layer. Compared to traditional thresholding, AI segmentation accurately delineates material phases and void spaces, enhancing the reproducibility and resolution of morphological assessments. The results demonstrate that compaction-induced reductions in porosity and thickness strongly impact membrane transport properties. These findings provide mechanistic insights into the compaction behavior of RO membranes and underscore the potential for advanced imaging and AI-driven data analysis to guide the design of next-generation membranes with improved mechanical resilience and operational longevity.

13 HYDRO ENERGY↗
DOE OSTI2015

Untangleing the effects of chain rigidity on the structure and dynamics of strongly adsorbed polymer melts

Here, we present a detailed analysis of coarse-grained molecular dynamics simulations of semiflexible polymer melts in contact with a strongly adsorbing substrate. We have characterized the segments in the interfacial layer by counting the number of trains, loops, tails and unadsorbed segments. For more rigid chains, a tail and an adsorbed segment (a train) dominate while loops are more prevalent in more flexible chains. The tails exhibit a non-uniformly stretched conformation akin to the polydispersed pseudobrush envisioned by Guiselin. To probe the dynamics of the segments we computed the layer z-resolved intermediate coherent collective dynamics structure factor, S(q, t, z), mean-square displacement of segments, and the 2nd Legendre polynomial of the time-autocorrelation of unit bond vectors, 2 [n i (t,z)•n i (0,z)]>. Our results show that segmental dynamics is slower for stiffer chains and there is a strong correlation between the structure and dynamics in the interfacial layer. There is no glassy layer, and the slowing down in dynamics of stiffer chains in the adsorbed region can be attributed to the densification and the more persistent layering of segments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Impact of Asymmetric Microstructure on Ion Transport in Ti 3 C 2 T x Membranes

Consolidation or densification of low-dimensional MXene materials into membranes can result in the formation of asymmetric membrane structures. Nanostructural (short-range) and microstructural (long-range) heterogeneity can influence mass transport and separation mechanisms. Short-range structural dynamics include the presence of water confined between the 2D layers, while long-range structural properties include the formation of defects, micropores, and mesopores. Herein, it is demonstrated that structural heterogeneity in Ti 3 C 2 T x membranes fabricated via vacuum-assisted filtration significantly affects ion transport. Higher ion permeabilities are achieved when the dense “bottom” side of the membrane, rather than the porous “top” side, faces the feed solution. Characterization of the membrane reveals distinct differences in flake alignment, surface roughness, and porosity across the membrane. In conclusion, the directional dependence on permeability suggests that one region of the membrane experiences stronger internal concentration polarization, potentially suppressing permeability through the porous side of the membrane.

MXene↗